CN109374804B - Chromatographic analysis method for propane product in methanol-to-olefin process production - Google Patents
Chromatographic analysis method for propane product in methanol-to-olefin process production Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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Abstract
The invention relates to the field of propane product detection, and discloses a chromatographic analysis method for a propane product in the process production of preparing olefin from methanol. The method is implemented in a gas chromatograph having dual detection channels, a first detection channel configured with a PLOT-Q capillary column and a FID detector, and a second detection channel configured with a HP-AL/S capillary column and a FID detector, the method comprising the steps of: (1) carrying out sample injection analysis on the standard gas by adopting a gas chromatograph; (2) establishing a correction table by using standard gas composition according to an area external standard quantitative method; (3) analyzing a propane product sample produced by the methanol-to-olefin process by adopting a gas chromatograph; (4) and (4) carrying out data analysis processing according to the analysis result obtained in the step (3) and the correction table. The method of the invention can accurately analyze the composition of the propane product, and comprehensively solves the problem of accurate quantitative analysis of the components of the propane related materials in the MTO process.
Description
Technical Field
The invention relates to the technical field of propane product component analysis, in particular to a chromatographic analysis method for a propane product in the process production of preparing olefin from methanol.
Background
With the development and refining of petroleum, propane is one of the main products, and in the olefin chemical industry using light hydrocarbon naphtha as the main cracking raw material, propane is also one of the main by-products. The components of these propane products are predominantly carbon one to carbon four hydrocarbons, substantially free of oxygenates. With the development and maturity of the industrial technology of Methanol To Olefin (MTO) in recent years, the source of propane is richer, but the propane produced in the MTO process chain contains 1-15% of dimethyl ether, 0.01-0.4% of acetaldehyde, 2-4% of cyclopropane, 40-90 ppm of propadiene and 50-200 ppm of propyne.
The current propane quality standards are: the industrial propane butane quality standard SH0553-93 (confirmed in 2000) is analyzed by the following method: in the two quality standards and analysis methods, the packed column chromatography is adopted to analyze the components of propane products in the petrochemical industry, but the components with the content of less than 0.1 percent and high-content dimethyl ether in the propane products produced by the MTO process chain cannot be analyzed. The gas chromatography method for determining the hydrocarbon composition of cracking C4 is improved by the latest revision of SH/T1141-2015 of Shanghai petrochemical institute, the detection of components with the content of less than 0.1 percent is improved, but dimethyl ether and acetaldehyde in a propane product produced by an MTO process cannot be analyzed.
Disclosure of Invention
The invention aims to solve the problem that dimethyl ether and acetaldehyde in a propane product produced by an MTO process cannot be analyzed in the prior art, and provides a chromatographic analysis method for the propane product produced by the methanol-to-olefin process.
In order to achieve the above object, the present invention provides a method for analyzing a propane product in a methanol to olefin process, wherein the method is implemented in a gas chromatograph having dual detection channels, the first detection channel is configured with a PLOT-Q capillary column and a FID detector, and the second detection channel is configured with an HP-AL/S capillary column and a FID detector, the method comprises the following steps:
(1) carrying out sample injection analysis on the standard gas by adopting the gas chromatograph;
(2) establishing a correction table by using standard gas composition according to an area external standard quantitative method;
(3) analyzing a propane product sample produced by the methanol-to-olefin process by adopting the gas chromatograph;
(4) and (4) carrying out data analysis processing according to the analysis result obtained in the step (3) and the correction table.
According to the chromatographic analysis method, a gas chromatograph (such as an Agilent 7890B chromatograph) with double detection channels is adopted, and a PLOT-Q capillary column and an HP-AL/S capillary chromatographic column (namely an aluminum trioxide capillary column) are respectively arranged in the two detection channels, so that the analysis of trace components in the propane rectification material in the MTO process controlled production operation is accurately realized, and the quality control analysis specified by the standard of the factory propane byproduct is completed, the content of the detected component reaches 1 ppm-100% (v/v), the existing industrial propane and butane quality standard SH-0553-93 (confirmed in 2000) is overcome, and the industrial propane and butane component chromatographic analysis method SH/T0614-95 is realized, the defects that the content of components less than 0.1 percent and the high content of dimethyl ether in the propane product produced by the MTO process cannot be analyzed; SH/T1141-2015 has the defect that dimethyl ether cannot be analyzed by gas chromatography for industrial hydrocarbon composition determination of cracking C4. The method can be used for delivery inspection and control sample analysis in the middle of production.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a chromatographic analysis method of a propane product in the process production of methanol-to-olefin, which is implemented in a gas chromatograph with double detection channels, wherein the first detection channel is provided with a PLOT-Q capillary column and a FID detector, and the second detection channel is provided with an HP-AL/S capillary column and a FID detector, and the method comprises the following steps:
(1) carrying out sample injection analysis on the standard gas by adopting the gas chromatograph;
(2) establishing a correction table by using standard gas composition according to an area external standard quantitative method;
(3) analyzing a propane product sample produced by the methanol-to-olefin process by adopting the gas chromatograph;
(4) and (4) carrying out data analysis processing according to the analysis result obtained in the step (3) and the correction table.
In the analysis method of the present invention, the temperature of the FID detector in the first detection channel and the second detection channel is 280 to 320 ℃, preferably 300 ℃.
In the analysis method of the invention, the PLOT-Q capillary column has the specification of 30m multiplied by 0.53mm multiplied by 40 um; the specification of the HP-AL/S capillary chromatographic column is 50m multiplied by 0.53mm multiplied by 15 um; the column flow rate is 4-8ml/min, preferably 6 ml/min.
In the analysis method of the invention, in the gas chromatograph, the front sample inlet is a shunt sample inlet, the rear sample inlet is a non-shunt sample inlet, and the temperature of the sample inlet is 240-260 ℃, preferably 250 ℃.
In the analysis method of the present invention, the standard gas comprises, by volume: 10% of propane, 0.1% of cyclopropane, 2% of propylene, 0.5% of isobutane, 0.5% of n-butane, 0.01% of propadiene, 0.5% of trans-2-butene, 0.5% of 1-butene, 0.5% of isobutene, 0.5% of cis-2-butene, 0.01% of isopentane, 0.01% of n-pentane, 0.5% of 1.3 butadiene, 0.05% of propyne, 3% of dimethyl ether, 0.05% of acetaldehyde and the balance of nitrogen or helium.
In the analysis method, during the analysis process by adopting the gas chromatograph, the used carrier gas is nitrogen or helium; the combustion gas is hydrogen, and the hydrogen flow is 25-35ml/min, preferably 30 ml/min; the combustion-supporting gas is air, and the air flow is 380-420ml/min, preferably 400 ml/min; the flow rate of tail gas blowing is 20-30ml/min, preferably 25 ml/min.
In the analysis method according to the present invention, in the analysis using the gas chromatograph, the column temperature programming method is: the initial temperature is 35-45 deg.C, maintaining for 2-7min, increasing to 180-200 deg.C at a rate of 8-12 deg.C/min, and maintaining for 30-60 min; preferably, the initial temperature is 40 ℃ for 3min, and the temperature is raised to 190 ℃ at a heating rate of 10 ℃/min for 40 min.
In the analysis method of the present invention, in the step (4), the content of the target component is calculated according to the following formula during the data analysis processing,
Vi＝ai×fi
wherein Vi is the content of the target component in the sample, ai is the peak area of the corresponding target component in the sample measured in the step (3), and fi is a correction factor of the target component obtained by using standard gas.
The present invention will be described in detail below by way of examples. In the following examples, the reagents used were chosen according to the person skilled in the art as appropriate analytically or chromatographically pure products, all commercially available.
Example 1
(1) Gas chromatography conditions:
gas chromatograph: agilent 7890B gas chromatograph
A chromatographic column: column 1: PLOT-Q capillary column 30m × 0.53mm × 40um
Column 2: HP-AL/S capillary chromatographic column 50m × 0.53mm × 15um
Column temperature: maintaining at 40 deg.C for 3min, heating to 190 deg.C at a temperature rise rate of 10 deg.C/min, and maintaining for 40min
Column flow rate: 6ml/min
Sample inlet temperature: 250 deg.C
FID detector temperature: 300 deg.C
Carrier gas: high purity nitrogen
Hydrogen flow rate: 30ml/min
Air flow rate: 400ml/min
Flow rate of tail gas blowing: 25ml/min
The split ratio is as follows: 1:30
(2) Establishing a correction table
The standard gas volume percentage composition is: 10% of propane, 0.1% of cyclopropane, 2% of propylene, 0.5% of isobutane, 0.5% of n-butane, 0.01% of propadiene, 0.5% of trans-2-butene, 0.5% of 1-butene, 0.5% of isobutene, 0.5% of cis-2-butene, 0.01% of isopentane, 0.01% of n-pentane, 0.5% of 1.3 butadiene, 0.05% of propyne, 3% of dimethyl ether, 0.05% of acetaldehyde and the balance of nitrogen. And (4) measuring by using a gas chromatograph under the chromatographic conditions, and establishing a calibration table according to an external area standard quantitative method.
(3) And (3) analyzing an actual sample: : a300 ml pressure-resistant stainless steel cylinder is connected with a quick joint to obtain a propane product with a known composition, and the volume percentage of the propane product is as follows: 12% of propane, 0.05% of isopentane, 0.05% of n-pentane, 0.05% of propyne, 4% of dimethyl ether and the balance of nitrogen.
(4) Data report processing
The concentration of each target component in the propane product is calculated according to the following formula,
Vi＝ai×fi
vi.
a..... peak area of the corresponding target component in the propane product determined in step (3)
fi.
The volume percentage of the propane product obtained by calculation is as follows: 12.005% of propane, 0.049% of isopentane, 0.051% of n-pentane, 0.053% of propyne and 3.998% of dimethyl ether.
Therefore, the chromatographic analysis method can accurately analyze the composition of the propane product, and comprehensively solve the problem of accurate quantitative analysis of the components of the propane related materials in the MTO process.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (6)
1. A chromatographic analysis method for propane products in the methanol-to-olefin process production is characterized in that the method is implemented in a gas chromatograph with double detection channels, wherein the first detection channel is provided with a PLOT-Q capillary chromatographic column and a FID detector, and the second detection channel is provided with an HP-AL/S capillary chromatographic column and a FID detector, and the method comprises the following steps:
(1) carrying out sample injection analysis on the standard gas by adopting the gas chromatograph;
(2) establishing a correction table by using standard gas composition according to an area external standard quantitative method;
(3) analyzing a propane product sample produced by the methanol-to-olefin process by adopting the gas chromatograph;
(4) performing data analysis processing according to the analysis result obtained in the step (3) and the correction table;
wherein, the volume percentage composition of the standard gas is as follows: 10% of propane, 0.1% of cyclopropane, 2% of propylene, 0.5% of isobutane, 0.5% of n-butane, 0.01% of propadiene, 0.5% of trans-2-butene, 0.5% of 1-butene, 0.5% of isobutene, 0.5% of cis-2-butene, 0.01% of isopentane, 0.01% of n-pentane, 0.5% of 1, 3-butadiene, 0.05% of propyne, 3% of dimethyl ether and 0.05% of acetaldehyde;
in the process of analyzing by adopting the gas chromatograph, the temperature programming mode of the chromatographic column is as follows: maintaining the initial temperature at 35-45 deg.C for 2-7 min; heating to 180-200 deg.C at a temperature rising rate of 8-12 deg.C/min, and maintaining for 30-60 min.
2. The analytical method of claim 1, wherein the FID detector has a temperature of 280-320 ℃ in the first detection channel and the second detection channel.
3. The assay of claim 1, wherein the PLOT-Q capillary column has a specification of 30m x 0.53mm x 40um and the HP-AL/S capillary column has a specification of 50m x 0.53mm x 15 um; the column flow rate was 4-8 ml/min.
4. The analytical method of claim 1, wherein in the gas chromatograph, the front sample inlet is a split sample inlet, the rear sample inlet is a non-split sample inlet, and the sample inlet temperature is 240-260 ℃.
5. The analytical method according to claim 1, wherein, in the analysis using the gas chromatograph, a carrier gas used is nitrogen or helium; the combustion gas is hydrogen, and the hydrogen flow is 25-35 ml/min; the combustion-supporting gas is air, and the air flow is 380-420 ml/min; the flow rate of tail gas blowing is 20-30 ml/min.
6. The analytical method according to claim 1, wherein in the step (4), the target component content is calculated in the data analysis processing according to the following formula,
Vi＝ai×fi
wherein Vi is the content of the target component in the sample, ai is the peak area of the corresponding target component in the sample determined in the step (3), and fi is a correction factor of the target component obtained by using the standard sample.
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